CN108996636B - 一种聚硅磁性膨润土絮凝剂的制备方法 - Google Patents
一种聚硅磁性膨润土絮凝剂的制备方法 Download PDFInfo
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C02F1/00—Treatment of water, waste water, or sewage
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Abstract
本发明涉及一种利用粘土尾矿制备聚硅磁性膨润土的方法,将尾矿中有用成分膨润土经提纯分离后,添加磁性铁吸附制备磁性土,利用水热合成制备聚硅酸土备用,再将合成的聚硅酸土与磁性土进行复合,制备聚硅磁性膨润土絮凝剂。为该领域复合絮凝剂研究提供理论数据支持;未来开发无机高效聚合物改性粘土具有可观的应用价值;并且磁性复合絮凝剂的研究与开发,具有很好的现实意义。
Description
技术领域
本发明属于絮凝剂的制备领域,具体涉及一种聚硅磁性膨润土絮凝剂的制备方法。
背景技术
目前,絮凝剂按化学成分可以分为无机、有机、微生物和复合絮凝剂四大类。无机絮凝剂包括无机低分子絮凝剂(如传统铁盐、铝盐絮凝剂)和在此基础上发展起来的无机高分子絮凝剂。有机絮凝剂分为人工合成和天然的两种,其中人工合成有机高分子絮凝剂主要包括聚丙胺类等。絮凝剂种类繁多,都能产生一定的絮凝效果,但单一絮凝剂处理方法往往不如复合絮凝剂处理效果理想。而且有机絮凝剂存在难以生物降解、价格昂贵等缺陷,其单独应用受到了一定的限制。传统絮凝剂也会有容易残留的缺点,造成水体的二次污染。由于上述这些问题的存在,故在实际应用中可以将两种或两种以上的絮凝剂产品联合使用,利用其协同作用,提高混凝工艺单元的净水效果。
磁分离水处理技术是从矿物磁选技术发展而来,具有工艺简单、高效、无二次污染的特点,已广泛应用于钢铁废水等含有强磁性介质的废水处理,将絮凝剂和磁种结合用于不含磁性介质的水污染治理,成为近年来污染治理关注的热点。聚硅酸铁是目前研制的一种无机高效复合絮凝剂,具有成本低廉、絮凝效果好等特点,具有很好的应用前景。改性粘土也可用作絮凝剂,具有来源广泛、性能稳定、操作简单等特点,使用安全、绿色环保使其成为极具潜力和希望的复合絮凝剂之一。
与传统的CPAM絮凝剂相比,磁性絮凝剂具有用量少,分离过程快等优点,同时克服了传统絮凝剂易残留的缺点,有效避免了水体的二次污染。磁性絮凝剂除具有稳定的磁性外,还需要保持较好的絮凝特性,在其絮凝沉降过程中,可通过外磁分离技术实现絮体与水的分离。目前磁性絮凝剂一般都是以磁铁矿为磁颗粒,并且只能用于含铁废水处理。关于磁性絮体的聚集、吸附、沉降特性等基础研究较少。本研究将磁性铁与无机硅胶和天然粘土结合起来,增强改性效果形成磁性硅胶粘土絮凝剂,聚合的硅胶和粘土的交联多孔结构可以吸附金属离子和悬浮物,利用磁性特点进行快速分离。
发明内容
本研究针对聚硅酸磁性铁和改性粘土的特点,制备聚硅磁性膨润土絮凝剂,为该领域复合絮凝剂研究提供理论数据支持;在未来开发无机高效聚合物改性粘土具有可观的应用价值;并且磁性复合絮凝剂的研究与开发,具有很好的现实意义。发明涉及一种利用粘土尾矿制备聚硅磁性膨润土的方法,将尾矿中有用成分膨润土经提纯分离后,添加磁性铁吸附制备磁性土,利用水热合成制备聚硅酸土备用,再将合成的聚硅酸土与磁性土进行复合,制备聚硅磁性膨润土絮凝剂,利用模拟含铜废水进行吸附实验。
简单的工艺步骤与条件如下:
① 以Fe2+和Fe3+的物质的量比例为1:2-3:4,称取氯化铁和氯化亚铁共30g加水100ml配制混合溶液,使用1mol/L氢氧化钠溶液滴定调节pH值到11-12,反应温度80℃下不断搅拌,水浴加热30-60min,制备生成四氧化三铁磁性流体备用;
② 将①中磁性铁流体倒入搅拌槽中,加入10g膨润土粉搅拌30min,静置90min,除去上清液,制得磁性膨润土备用;
③ 称取10g九水合硅酸钠和10g膨润土粉,加90ml水混合搅拌均匀,配成悬浮液;利用适量1mol/L的盐酸缓慢滴定调节溶液pH值,不断搅拌,直至pH值转变为6-7,静置60min使其聚合,制备得聚合硅酸粘土;
④ 以Fe:Si=5:1的摩尔比向③中聚合硅酸粘土悬浮液中加入氯化亚铁,用1mol/L的氢氧化钠溶液调节溶液的pH值为7-8;
⑤ 将②和④制得产物混合;放进恒温加热磁力搅拌器,在50℃-80℃下水浴加热,同时磁力搅拌聚合30min,静置60min后将溶液进行抽滤脱水得到聚硅磁性膨润土絮凝剂。
步骤②和③中所用膨润土粉为提出后的膨润土粉,提纯方法为:
a. 将原矿样在制样机中进行研磨,五分钟取出样品,用200目筛子进行筛分,筛上产品继续研磨筛分,得到200目的矿样;
b. 将磨细后的矿样制成10%溶液,倒入搅拌槽中进行2h搅拌,将上层清液和中间的精矿抽取出来,将沉砂除去,提纯干燥后待用。
产品的使用方法:本絮凝剂使用方便,回收简单。只需按用量称取适量制备好的磁性粘土矿物材料,即本絮凝剂,倒入待处理溶液中进行吸附;吸附30-120分钟后,利用外磁场或磁铁吸出分离污染物,去除溶液中金属离子或浑浊物,水体即可得到处理。使用过的承载污染物的絮凝剂用稀酸液清洗即可再次使用。
本发明的有益效果:
本絮凝剂具有用量少,分离过程快等优点,同时克服了传统絮凝剂易残留的缺点,有效避免了水体的二次污染。并具有稳定的磁性,还可保持较好的絮凝特性,在其絮凝沉降过程中,可通过外磁分离技术实现絮体与水的分离。可应用于各种重金属污染、水环境富营养化、水体浑浊等水处理以及环境治理应用领域。
本研究将磁性铁与无机硅胶和天然粘土结合起来,增强改性效果形成磁性硅胶粘土絮凝剂,聚合的硅胶和粘土的交联多孔结构可以吸附金属离子和悬浮物,利用磁性特点进行快速分离。
附图说明
图1为磁性膨润土展示图;
图2为膨润土原矿的红外光谱图;
图3为聚硅磁性膨润土红外光谱图;
图4为吸附铜离子后的聚硅磁性膨润土红外光谱图;
图5为膨润土原矿的XRD图谱;
图6为聚硅磁性膨润土XRD图谱;
图7为磁性膨润土SEM图谱;
图8为聚硅磁性膨润土SEM图谱。
具体实施方式
通过下述实施例将有助于理解本发明,但并不限制本发明的内容。
实施例1
一种聚硅磁性膨润土絮凝剂的制备方法,包括以下步骤:
① 以Fe2+和Fe3+的物质的量比例为2:3,称取氯化铁和氯化亚铁共30g加水100ml配制混合溶液,使用1mol/L氢氧化钠溶液滴定调节pH值到11,反应温度80℃下不断搅拌,水浴加热45min,制备生成四氧化三铁磁性流体备用;
② 将①中磁性铁流体倒入搅拌槽中,加入10g膨润土粉搅拌30min,静置90min,除去上清液,制得磁性膨润土备用;
③ 称取10g九水合硅酸钠和10g膨润土粉,加90ml水混合搅拌均匀,配成悬浮液;利用适量1mol/L的盐酸缓慢滴定调节溶液pH值,不断搅拌,直至pH值转变为6,静置60min使其聚合,制备得聚合硅酸粘土;
④ 以Fe:Si=5:1的摩尔比向③中聚合硅酸粘土悬浮液中加入氯化亚铁,用1mol/L的氢氧化钠溶液调节溶液的pH值为7;
⑤ 将②和④制得产物混合;放进恒温加热磁力搅拌器,在60℃下水浴加热,同时磁力搅拌聚合30min,静置60min后将溶液进行抽滤脱水得到聚硅磁性膨润土絮凝剂。
步骤②和③中所用膨润土粉为提出后的膨润土粉,提纯方法为:
a. 将原矿样在制样机中进行研磨,五分钟取出样品,用200目筛子进行筛分,筛上产品继续研磨筛分,得到200目的矿样;
b. 将磨细后的矿样制成10%溶液,倒入搅拌槽中进行2h搅拌,将上层清液和中间的精矿抽取出来,将沉砂除去,提纯干燥后待用。
图2为膨润土原矿的红外光谱图;图3为实施例1制备的聚硅磁性膨润土红外光谱图。由图2至3中样品中膨润土的强吸收波谱在高频区3487 cm-1、中频区1051cm-1、低频区498cm-1附近。在图上分别有Si-O键、Al-O键等的伸缩振动,说明是典型的蒙脱石矿物的红外光谱。由于Al-O-H的伸缩振动引起高频区3487 cm-1的变化,且吸附后峰形变尖锐。低频区501cm-1和498cm-1处,可以认为与膨润土的Si-O-Me(金属阳离子)和Me-O的偶合振动有关,推论Fe进入膨润土晶层吸附。800cm-1的单峰强度不同是由膨润土的Si-O-Fe弯曲振动引起的,样品中Fe含量的不同而导致单峰强度不同。改性后的磁性粘土矿物含有Fe-O键,通过测试结果可以推测,在改性前后,膨润土的层间结构发生了变化,吸附能力增强。
图5为膨润土原矿的XRD图谱;图6为实施例1制备的聚硅磁性膨润土XRD图谱。由图5至图6,通过上面XRD图谱可以看出,原矿的XRD图谱中,波峰尖锐,晶型明显较为完整。在经过制备得到的聚硅磁性膨润土的XRD衍射图谱中可以看出,峰形有明显坍塌,d001数值由1.2673nm增加为1.3753nm。其d001衍射峰发生轻微偏移,衍射峰强度显著降低,同时,出现了新的波峰,结合试验推论是四氧化三铁颗粒与改性硅酸负载在矿物上,在改性过程中,膨润土的层间结构发生了变化,四氧化三铁插入层间。
图7为磁性膨润土SEM图谱;图8为实施例1制备的聚硅磁性膨润土SEM图谱。由图7至图8,通过上面SEM图谱可以看出,磁性膨润土的SEM图谱中,层片结构明显,表面有部分杂质石英。聚硅磁性膨润土的表面吸附更多硅氧胶质,多孔结构更发育了,吸附能力增强。
实施例2
一种聚硅磁性膨润土絮凝剂的制备方法,包括以下步骤:
① 以Fe2+和Fe3+的物质的量比例为3:4,称取氯化铁和氯化亚铁共30g加水100ml配制混合溶液,使用1mol/L氢氧化钠溶液滴定调节pH值到11,反应温度80℃下不断搅拌,水浴加热30min,制备生成四氧化三铁磁性流体备用;
② 将①中磁性铁流体倒入搅拌槽中,加入10g膨润土粉搅拌30min,静置90min,除去上清液,制得磁性膨润土备用;
③ 称取10g九水合硅酸钠和10g膨润土粉,加90ml水混合搅拌均匀,配成悬浮液;利用适量1mol/L的盐酸缓慢滴定调节溶液pH值,不断搅拌,直至pH值转变为7,静置60min使其聚合,制备得聚合硅酸粘土;
④ 以Fe:Si=5:1的摩尔比向③中聚合硅酸粘土悬浮液中加入氯化亚铁,用1mol/L的氢氧化钠溶液调节溶液的pH值为8;
⑤ 将②和④制得产物混合;放进恒温加热磁力搅拌器,在50℃下水浴加热,同时磁力搅拌聚合30min,静置60min后将溶液进行抽滤脱水得到聚硅磁性膨润土絮凝剂。
步骤②和③中所用膨润土粉为提出后的膨润土粉,提纯方法为:
a. 将原矿样在制样机中进行研磨,五分钟取出样品,用200目筛子进行筛分,筛上产品继续研磨筛分,得到200目的矿样;
b. 将磨细后的矿样制成10%溶液,倒入搅拌槽中进行2h搅拌,将上层清液和中间的精矿抽取出来,将沉砂除去,提纯干燥后待用。
实施例3
一种聚硅磁性膨润土絮凝剂的制备方法,包括以下步骤:
① 以Fe2+和Fe3+的物质的量比例为1:2,称取氯化铁和氯化亚铁共30g加水100ml配制混合溶液,使用1mol/L氢氧化钠溶液滴定调节pH值到12,反应温度80℃下不断搅拌,水浴加热60min,制备生成四氧化三铁磁性流体备用;
② 将①中磁性铁流体倒入搅拌槽中,加入10g膨润土粉搅拌30min,静置90min,除去上清液,制得磁性膨润土备用;
③ 称取10g九水合硅酸钠和10g膨润土粉,加90ml水混合搅拌均匀,配成悬浮液;利用适量1mol/L的盐酸缓慢滴定调节溶液pH值,不断搅拌,直至pH值转变为6,静置60min使其聚合,制备得聚合硅酸粘土;
④ 以Fe:Si=5:1的摩尔比向③中聚合硅酸粘土悬浮液中加入氯化亚铁,用1mol/L的氢氧化钠溶液调节溶液的pH值为8;
⑤ 将②和④制得产物混合;放进恒温加热磁力搅拌器,在80℃下水浴加热,同时磁力搅拌聚合30min,静置60min后将溶液进行抽滤脱水得到聚硅磁性膨润土絮凝剂。
步骤②和③中所用膨润土粉为提出后的膨润土粉,提纯方法为:
a. 将原矿样在制样机中进行研磨,五分钟取出样品,用200目筛子进行筛分,筛上产品继续研磨筛分,得到200目的矿样;
b. 将磨细后的矿样制成10%溶液,倒入搅拌槽中进行2h搅拌,将上层清液和中间的精矿抽取出来,将沉砂除去,提纯干燥后待用。
含铜废水的吸附实验
成功制备得到聚硅磁性膨润土絮凝剂后,对溶液中离子的吸附性能进行应用,选用浓度为0.5g/L的铜离子溶液进行吸附试验。并用可见光分光光度计进行测试。测试时使用如下方法来测试经聚硅磁性膨润土絮凝剂吸附后的铜离子溶液的浓度。
测试铜离子浓度的步骤:
配制试剂:
1、配制柠檬酸铵溶液置于容量瓶中;
2、使用氯化铵和氢氧化铵配制氢氧化铵-氯化铵缓冲溶液,称量40g氯化铵,移取40mL密度为0.9g/mL的氢氧化铵,溶解后倒入容量瓶,用水稀释到1L,摇匀;
3、配制双环己酮草酰二腙(B.C.O)溶液:称取2gB.C.O溶解于500mL热水和500mL乙醇中,溶解后置于1L容量瓶,用水稀释到刻度线,摇匀;
4、配制铜离子溶液(0.5g/L):称取0.5g五水硫酸铜,溶解于水中,倒入1L容量瓶,用水稀释到刻度线,摇匀。
测试步骤:
1)移取50mL配制好的0.5g/L的铜离子溶液于烧杯中;
2)称取实施例1中制备好的聚硅磁性膨润土絮凝剂,倒入溶液中进行吸附试验;
3)吸附30分钟后,移取上清液10mL于烧杯中,分别加入5mL柠檬酸铵溶液,10mL氢氧化铵-氯化铵缓冲溶液,5mLB.C.O溶液;
4)将3)中溶液移到50mL容量瓶中,用水稀释到刻度线,摇匀,静置8分钟;
5)移取少量4)中溶液至比色皿中,放置于分光光度计在,在610nm波长处进行测试。
制得的产物用铜离子吸附试验吸附后得到如表1的数据
表1
由表中数据可知,用量在0.2-1g/L本絮凝剂均取得较好的吸附效果,以0.6g/L投加量时,表现出更好的吸附效果,去除铜离子效果明显。
图4为吸附铜离子后的聚硅磁性膨润土红外光谱图。
以上所述仅为本发明的较佳实施例,凡依本发明申请专利范围所做的均等变化与修饰,皆应属本发明的涵盖范围。
Claims (2)
1.一种聚硅磁性膨润土絮凝剂的制备方法,其特征在于,包括以下步骤:
①以Fe2+和Fe3+的物质的量比例为1:2-3:4,称取氯化铁和氯化亚铁共30g加水100ml配制混合溶液,使用1mol/L氢氧化钠溶液滴定调节pH值到11-12,反应温度80℃下不断搅拌,水浴加热30-60min,制备生成四氧化三铁磁性流体备用;
②将①中磁性铁流体倒入搅拌槽中,加入10g膨润土粉搅拌30min,静置90min,除去上清液,制得磁性膨润土备用;
③称取10g九水合硅酸钠和10g膨润土粉,加90ml水混合搅拌均匀,配成悬浮液;利用适量1mol/L的盐酸缓慢滴定调节溶液pH值,不断搅拌,直至pH值转变为6-7,静置60min使其聚合,制备得聚合硅酸粘土;
④以Fe:Si=5:1的摩尔比向③中聚合硅酸粘土悬浮液中加入氯化亚铁,用1mol/L的氢氧化钠溶液调节溶液的pH值为7-8;
⑤将②和④制得产物混合;放进恒温加热磁力搅拌器,在50℃-80℃下水浴加热,同时磁力搅拌聚合30min,静置60min后将溶液进行抽滤脱水得到聚硅磁性膨润土絮凝剂。
2.根据权利要求1所述的一种聚硅磁性膨润土絮凝剂的制备方法,其特征在于,步骤②和③中所用膨润土粉为提纯 后的膨润土粉,提纯方法为:
a. 将原矿样在制样机中进行研磨,五分钟取出样品,用200目筛子进行筛分,筛上产品继续研磨筛分,得到200目的矿样;
b. 将磨细后的矿样制成10%溶液,倒入搅拌槽中进行2h搅拌,将上层清液和中间的精矿抽取出来,将沉砂除去,提纯干燥后待用。
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